반응 #92991

반응 방정식

16β-ethyl-17β-bromoacetoxy-4-estren-3-one

n-octanoic acid

→

above-identified compound

16β-Ethyl-17β-n-octanoyloxyacetoxy-4-estren-3-one

용매

acetone

NaOH

water

반응 조건

후처리

1. 1
   workup.ADDITIONare serially added to the above solution
2. 2
   온도The mixture is refluxed for 4 hours
3. 3
   workup.DISTILLATIONThe solvent is distilled off under reduced pressure
4. 4
   추출the residue is extracted with 150 ml of ethyl acetate
5. 5
   기타The organic layer is separated
6. 6
   세척washed with water and saturated aqueous sodium chloride solution
7. 7
   건조dried over anhydrous magnesium sulfate
8. 8
   workup.DISTILLATIONThe solvent is then distilled off under reduced pressure
9. 9
   세척passage of 50 ml of diisopropyl ether, elution
10. 10
    기타The eluate is evaporated under reduced pressure
11. 11
    기타to remove the solvent

실험 절차

In 60 ml of acetone is dissolved 1.0 ml of n-octanoic acid, and 3.0 ml of 2N-NaOH, 15 ml of water and 1.8 g of 16β-ethyl-17β-bromoacetoxy-4-estren-3-one are serially added to the above solution. The mixture is refluxed for 4 hours. The solvent is distilled off under reduced pressure and the residue is extracted with 150 ml of ethyl acetate. The organic layer is separated, washed with water and saturated aqueous sodium chloride solution and dried over anhydrous magnesium sulfate. The solvent is then distilled off under reduced pressure and the residue is subjected to column chromatography. Following passage of 50 ml of diisopropyl ether, elution is carried out with 300 ml of the same solvent. The eluate is evaporated under reduced pressure to remove the solvent, giving 1.7 g of the above-identified compound as a colorless oil.

출처